American Journal of Analytical Chemistry, 2011, 2, 235-242
doi:10.4236/ajac.2011.22028 Published Online May 2011 (http://www.SciRP.org/journal/ajac)
Copyright © 2011 SciRes. AJAC
Liquid Chromatographic Determination of Scopolamine in
Hair with Suspended Drop Liquid Phase
Microextraction Technique
Mahboubeh Masrournia
1*
, Zarrin Es’haghi
2
, Mostafa Amini
1
1
Department of Chemistry, Faculty of Sciences, Mashhad Branch, Islamic Azad University, Mashhad, Iran
2
Department of Chemistry, Faculty of Sciences, Payam Noor University, Tehran, Iran
E-mail: masrournia@yahoo.com, masrour@mshdiau.ac.ir
Received December 3, 2010; revised March 10, 2011; accepted March 14, 2011
Abstract
Hair analysis is used in some branches of alternative medicine as a method of investigation to assist
diagnosis. It is very useful when a history of drug use is difficult or impossible to obtain. In this research
suspended droplet liquid phase microextraction (SDLME) coupled with high-performance liquid chroma-
tography and photodiode array detection (HPLC-DAD) was used for preconcentration and analysis of sco-
polamine in hair samples. Therefore scopolamine was extracted from 2.0 g hair sample incubated in metha-
nol (5 h, 50˚C) and adjusted to pH 7.4 with, Na
2
HPO
4
–H
3
PO
4
buffer solution (donor phase, P
1
) into an or-
ganic phase (P
2
) 350 μl n-octanol and then back extracted into a micro drop of aqueous acceptor phase (P
3
),
adjusted at pH 3, with HCL. The extraction time, T
1
(from P
1
to P
2
) was 2 min and T
2
(from P
2
to P
3
) was 30
min. Optimum instrumental conditions were included; A C
18
reverse phase column with water-acetonitrile-
methanol (80:10:10) as the mobile phase was used and wavelength for UV detection was 205 nm. The linear
range was 10 to 10000 ng·mL
–1
, enrichment factor, detection limit and relative standard deviation were 77,
0.1 ng·mL
–1
and 5.4 respectively.
Keywords: Column Liquid Chromatography, Directly Suspended Droplet Liquid Phase Microextraction
(SDLME), Scopolamine, Hair Sample
1. Introduction
Tropane alkaloids such as atropine and scopolamine
(Figure 1) are muscarinic antagonists that block neu-
ron-transmission across muscarinic cholinergic receptors.
The toxicity of these drugs has been well known for
centuries and has been linked to poisoning and death,
usually due to heart or respiratory failure. Scopolamine
was shown toxic effects on central and peripheral nerv-
ous system [2]. Besides an increase of recreational abuse
[3], scopolamine has been occasionally used for its seda-
tive properties.
Tropane alkaloid determination in biological samples
such as serum, blood, urine and hair has a significant
importance in poisoning and forensic case [4]. Moreover
hair analysis is a new perspective in forensic toxicology
[5,6].
Hair may be considered for retrospective purposes
when blood and urine are no longer expected to contain a
particular contaminant, typically a year or less. Its most
widely accepted use is in the fields of forensic toxicology
and environmental toxicology. Several alternative medi-
cine fields also use various hair analysis for environ-
mental toxicology but these uses are controversial and not
standardized [7] But, drug determination in the human
Figure 1. Structure of the scopolamine and its pKa and log
Po/w values [1].